Effect of Ni addition on the densification of TiC: A comparative study of conventional and microwave sintering

This study deals with the effect of conventional sintering and microwave sintering on the densification kinetics of Titanium Carbide (TiC) in the presence of Ni (1, 1.5, 2 wt%). TiC compacts were obtained after uniaxial pressing of powders synthesised by ball milling of Titanium and Carbon and sintering was done in the presence of Nickel. The samples prepared were subjected to conventional as well as microwave sintering. The XRD and SEM analysis were used for a study of the reaction of Ti and C powders upon addition of Ni, which reduced the sintering temperature to 1200 °C. The densification of TiC powders was due to the Ti-Ni eutectic system, the liquid phase formed at this temperature assisting the sintering process. The SEM images revealed the flake like structure of TiC in which the carbon diffused into Ti upon the addition of Ni, thereby supporting enhanced mass transfer. The XRD pattern showed the presence of Titanium Oxide (TiO₂) along with TiC which resulted in non-uniform distribution of hardness. Maximum hardness was achieved in the conventional sintered compacts which gradually increased with increase in Ni addition. The presence of the oxide phase and the formation of micro cracks resulted in non-uniform hardness for microwave sintered compacts. The maximum hardness of conventional sintered compact (375 HLD) was nearly 1.5 times more than the maximum hardness of the microwave sintered compact (250 HLD). The density of the microwave sintered compact was found to be higher by 8% than with the conventionally sintered compact.     

合金元素P,Cu含量对铸铁短纤维结合剂组织和性能的影响

本文研究了合金元素磷和铜对铸铁短纤维烧结体显微组织和性能的影响。结果表明，合金元素磷可显著提高铸铁短纤维烧结体的密度、致密化系数和压强度。磷与铜的共同加入可进一步提高烧结体的压溃强度和硬度，同时，铜的加入可抑制由磷引起的烧结体的急剧。烧结机理随磷、铜含量的增加逐渐由固相烧结＋瞬态液烧结转变为液相烧结。     

Solid state and liquid phase sintering of mechanically activated W–20 wt.% Cu powder mixture

W–20 wt.% Cu powder mixture was mechanically alloyed by high-energy ball milling for various times and the effect of mechanical alloying (MA) on the sintering response of the composite compacts was investigated. The densification, microstructure, hardness and electrical conductivity after solid phase sintering (SPS) and liquid phase sintering (LPS) were examined. It was shown that the microstructure of mechanically alloyed powder profoundly influence the sintering response, i.e. a meaningful relationship between the sintering kinetics and the milling time was observed. It is suggested that MA disintegrates the W–W particle networks and increases the contribution of solid phase sintering (SPS) of nanostructured Cu and W particles on the densification. Higher hardness and conductivity were achieved by prolonged MA and SPS, indicating a lower W–W contiguity of the milled powders compared with the conventionally prepared W–Cu composite. On the other hand, depression of the melting temperature of copper up to 145 °C was noticed by affording a prolonged MA. The lower melting temperature and finer distribution of the Cu particles in the W matrix enhanced the densification during LPS and improved the homogeneity and properties of the final product.     

Magnetic properties of nanocrystalline Ni3Fe compacts prepared by spark plasma sintering

Nanocrystalline Ni₃Fe compacts were successfully prepared by spark plasma sintering starting from wet mechanically alloyed powders. The influences of the sintering conditions: sintering temperature, sintering time and particle size on the compact magnetic properties are investigated. It is found that high sintering temperature, increased sintering duration and larger particle size leads to compacts with improved soft magnetic properties. A contamination with carbon of the compacts during the sintering processes has been found to reduce their magnetic properties. It is found that a heat treatment at the temperature of 450 °C during 4 h, in hydrogen atmosphere, leads to an improvement of the compact coercivity and of the maximum relative permeability of the compact to up to 600% and 50% respectively. Spark plasma sintering can consequently be considered as promising compaction technique for processing Ni₃Fe nanocrystalline powder in particular and nanocrystalline soft magnetic alloys in general.     

Densification behavior of nanocrystalline W–Ni–Fe composite powders prepared by sol-spray drying and hydrogen reduction process

This paper studied the densification behavior of nanocrystalline composite powders of 93W–4.9Ni–2.1Fe (wt.%) and 93W–4.9Ni–2.1Fe–0.03Y synthesized by sol-spray drying and hydrogen reduction process. The X-ray diffraction (XRD) analysis showed that γ-(Ni, Fe) phase was formed in the final obtained powders. Powders morphology characterized by scanning electron microscope (SEM) showed that the 93W–4.9Ni–2.1Fe nanocrystalline composite powders exhibited larger agglomeration and grain size compared with the 93W–4.9Ni–2.1Fe–0.03Y nanocrystalline composite powders. Both kinds of green compacts can obtain full density if sintered at 1410 °C for 1 h. When sintering temperature was above 1410 °C, the sintering density for both compacts decreased rapidly. In addition, the sintering density, densification rate and grain coarsening rate of 93W–4.9Ni–2.1Fe compacts were higher than those of 93W–4.9Ni–2.1Fe–0.03Y. The effect of trace yttrium on the densification behavior of nanocrystalline composite powders was also discussed.     

烧结温度对Micro-FAST制备钛微型齿轮致密化的影响

将新颖的多物理场活化烧结微成形技术(Micro-FAST)引入到钛微型齿轮的制备中,研究了烧结温度对Micro-FAST制备钛微型齿轮致密化的影响。结果表明,在1200℃烧结保温4 min,体系的相对密度即可达到90.5%。Micro-FAST的烧结致密化过程大致可分为4个阶段:预热阶段、低温保温阶段、快速升温阶段和烧结保温阶段,钛粉末的致密化过程主要发生在快速升温阶段。对烧结体系的收缩动力学曲线研究发现,在电场、力场和温度场的耦合作用下,粉末体系在450℃发生了塑性变形,在1032℃生成了局部液相。研究表明,与传统烧结法相比,多物理场活化烧结法是一种新型和高效的制备钛微型零件的良好方法。     

The influence of percolation during pulsed electric current sintering of ZrO2–TiN powder compacts with varying TiN content

A series of ZrO₂–TiN composite powder compacts with varying TiN content was densified using the field assisted sintering technique, also known as spark plasma sintering or pulsed electric current sintering (PECS). The TiN content was varied between 35 and 90 vol.% in order to obtain an electrical conductive composite material that can be shaped by electrical discharge machining. The influence of the TiN content on the densification behaviour was investigated experimentally, whereas its influence on the temperature and current distribution in the PECS tool set-up was simulated using a previously developed finite element model. The predicted temperature distribution was confirmed experimentally using a double pyrometer set-up, one focusing on the outer die wall surface and one on the bottom of a borehole in the upper punch. The changing thermal and electrical properties of the sintering ZrO₂–TiN powder compacts were calculated using mixture rules. Using a double pyrometer set-up, a clear relationship could be verified experimentally between the changing electrical properties of the sintering compact and the temperature redistribution in the punch/die/sample set-up during the PECS process. The homogeneity of sintering inside the PECS equipment is discussed in detail and suggestions are made in order to promote a more homogeneous sintering process. Carbon felt, acting as a thermal insulator, was placed around the die in order to minimize the radiation heat losses and to minimize the thermal gradients during heating and the dwell period at maximum temperature. The mechanical and electrical properties of the different composite materials are discussed as functions of the TiN content.     

Effects of lubrication and aspect ratio on the consolidation of metal matrix composites under cyclic pressure

The effects of powder compaction under cyclic load were compared to traditional single-cycle compaction. The effect of interparticle friction as modified by lubrication and compact aspect ratio received particular attention. Mixtures of Al and Al₂O₃ were consolidated at room temperature in contained uniaxial consolidation experiments. The experiments showed that in static compaction, lubrication aids densification at low pressures but can inhibit consolidation at high pressures. Enhanced densification was observed following pressure cycling. These improvements were more pronounced in compacts having smaller aspect ratios. The efficiency of pressure cycling was reduced by the lubricant. Lubrication also decreased the effects of aspect ratio in both the static and cyclic compaction cases. Although lubrication did increase density uniformity, the resulting compact green strength was much lower. Both single and double action compaction were studied and the best green strength and density distribution were obtained with double-action compaction under cyclic pressure without lubricant.     

Microstructure evolution and densification kinetics of Al2O3/Ti(C,N) ceramic tool material by microwave sintering

The microstructure evolution and densification kinetics of Al₂O₃/Ti(C,N) ceramic tool material during microwave sintering were studied. The density and grain growth significantly increases at the temperatures higher than 1400 °C. The calculated kinetics parameter n indicates that volume diffusion is the main densification mechanism when the sintering temperature is below 1300 °C, while grain boundary diffusion plays a leading role in the densification process when the sintering temperature is higher than 1300 °C. The grain growth activation energy of Al₂O₃/Ti(C,N) composite is 48.82 KJ/mol, which is much lower than those of monolithic Al₂O₃ in the microwave sintering and conventional sintering. The results suggested that the Al₂O₃/Ti(C,N) ceramic tool material with nearly full densification and fine grains can be prepared by two-step microwave sintering.     

Effects of rare earth addition on sintering process and dielectric property of cordierite based glass-ceramics

The effects of rare earth oxide on the sintering and dielectric property of cordierite-based glass-ceramics with non-stoichiometric composition prepared by quenching of molten droplets were investigated. The results show that the addition of rare earth oxide can lower the sintering temperature of cordierite glass-ceramics, improve the densification process and obviously reduce sintering activation energy. It is found that the densification of cordieritebased glass-ceramics is a liquid phase sintering process. The dielectric constant of the sintered compacts enhances with the increase of the density. When the sintering temperature is identical, the rare earth addition is found to have a noticeable effect on the dielectric loss of glass-ceramics. The properties of the glass-ceramics containing rare earth oxide appear to be correct for low firing temperature substrates.     

Effect of heating mode and sintering temperature on the consolidation of 90W-7Ni-3Fe alloys

The present study compares the sintering response of 90W-7Ni-3Fe alloys consolidated in a 2.45 GHz microwave furnace and a conventional furnace. The W-Ni-Fe compacts were sintered in a temperature range of 1200-1500 °C corresponding to solid-state as well as liquid phase sintering. The compacts were successfully sintered in a microwave furnace with about 80% reduction in the overall processing time. For both the heating modes, the W-Ni-Fe alloys exhibited significant densification prior to melt formation through solid-state sintering. The in situ dilatometric studies revealed that the contribution to densification from solid-state sintering is higher at lower heating rates. In comparison to conventional sintering, microwave sintered compacts showed relatively refined microstructure and higher hardness and flexural strength.     

Synthesis and consolidation of γ-Ni-Fe nanoalloy powder

The present work studies the synthesis and consolidation of γ-Ni-Fe nanoalloy powder by the mechano-chemical process comprising high-energy ball-milling of NiO-Fe₂O₃ powder and a subsequent hydrogen reduction process. To examine the formation mechanism of the nanoalloy powder, the effect of the oxide powder char-acteristics on the reduction process and alloying was investigated by varying the ball-milling time. The reduction process and the alloying of the γ-Ni-Fe phase proved to accelerate as the ball-milling time increased. However, prolonged milling (for 30 hours) retarded the reduction of Fe₂O₃ as well as the alloying process. The densification process of the Ni-Fe nanoalloy powder strongly depended on the degree of agglomeration which results in enhancing homogeneous sintering. The limited densification of the nanoalloy powder originates from the high degree of particle agglomeration. While intra-agglomerate porosity is easily eliminated in the course of sintering, it is found to resist densification. The limitation of the sintered density could be overcome by increasing the green density of the powder compacts. Full density was achieved by starting with a green density of 72% theoretical density.     

Microstructural evolution during sintering of near-monosized agglomerate-free submicron alumina powder compacts

Colloidally processed near-monosized, agglomerate-free submicron alumina powder compacts were sintered under different conditions to study the evolution of pore structures during sintering. The results showed that even though the compacts were agglomerate-free to start with, agglomeration took place during sintering due to local densification of the particles with different co-ordination numbers. Inter-agglomerate channel-like pores were formed as a result, which eventually evolved into an isolated pore on further sintering. The densification rate was controlled by mass transport via grain boundary diffusion before the formation of isolated inter-agglomerate pores, after which it was controlled by the sinterability of the pores. From this stage on, grain growth was required to bring about further sintering. At low sintering temperatures, grain growth was sluggish, probably a result of impurity controlled grain growth. This resulted in an abrupt drop in the densification rate and the phenomenon of end density at low sintering temperatures. The present work shows that an initial agglomerate-free green structure of fine, monosized particles is essential to resist particle agglomeration and grain growth during sintering, so as to achieve a low sintering temperature and a fine grain size sintered product.     

Effect of graphene nano-platelet addition on the microstructure and spark plasma sintering kinetics of zirconium diboride

In this paper, the effect of graphene nano-platelet (GNP) addition on the microstructure and sintering kinetics of ZrB₂ during spark plasma sintering (SPS) is presented. SPS was carried out at 1800 °C temperature and 50 MPa pressure. GNP addition resulted in an increase in the relative density from 84% to 97%. Retention of GNPs after SPS was confirmed through Scanning Electron Microscopy (SEM) and Energy Dispersive Spectroscopy (EDS) in conjunction with X-ray diffraction (XRD) and Raman spectroscopy. The effect of GNP reinforcement on sintering kinetics, microstructure and mechanical properties (Vickers micro hardness and indentation fracture toughness) are discussed. The ZrB₂ -GNP samples showed different activation energies at different temperature ranges which are explained based on the likely processes that are involved during sintering. Final stage of sintering exhibited lower activation energy during which the GNP aided grain boundary sliding enhancing the densification. Several toughening mechanisms such as GNP fracture, GNP shearing, GNP bending and GNP pullout were observed.     

Effects of Kaolinite addition on the densification and dielectric properties of BaTiO3 ceramics

Commercial Kaolinite was employed as sintering aid to reduce the sintering temperature of BaTiO₃ ceramics. The effects of Kaolinite content and sintering temperature on the densification, microstructure and dielectric properties of BaTiO₃ ceramics have been investigated. The density characterization results show that the addition of Kaolinite significantly lowered the sintering temperature of BaTiO₃ ceramics to about 1200 °C. XRD results show BaTiO₃ ceramics with a low amount of Kaolinite exhibited perovskite structure, but 10.0 wt% Kaolinite additions resulted in the formation of a secondary phase, BaAl₂Si₂O₈. BaO-TiO₂-Al₂O₃-SiO₂ glass phase was formed and improved the average breakdown strength of ceramics, which was supported by SEM-EDX results. The Kaolinite content had shown a strong influence on the dielectric constant and the diffuse transition. BaTiO₃ ceramic with 4.0 wt% Kaolinite addition possessed well temperature stability of dielectric constant.     

Sintering response of austenitic (316L) and ferritic (434L) stainless steel consolidated in conventional and microwave furnaces

This study compares the effect of heating mode on the densification, microstructure, strength and hardness of austenitic and ferritic stainless steel. The compacts were sintered in a radiatively heated (conventional) and a 2.45 GHz microwave furnace. Both 316L and 434L compacts couple with microwaves and heat up to the sintering temperature rapidly (45 °C/min). The overall processing time was reduced by about 90% through microwave sintering. While the microwave sintered compacts exhibit a finer microstructure, there is no corresponding improvement in densification and mechanical properties. This has been correlated with elongated and irregular pore structure.     

Mechanical properties of spark plasma sintered Nb–Al compacts strengthened by dispersion of Nb2N phase and additions of Mo and W

Mechanically alloyed and blended Nb–Al–N powders were sintered by the spark plasma sintering process, and their microstructure and mechanical properties were investigated. All of the Nb–Al–N compacts consisted of phases in the Nb–Al system in which the Nb₂N phase was dispersed. The microstructure of blended powder compacts was much coarser than that of mechanically alloyed powder compacts. The compacts obtained by sintering powder produced by crushing blended powder compacts have finer microstructure, higher hardness, and higher fracture toughness than blended powder compacts. The strength of Nb–Al–N compacts increases with increasing the fraction of AlN added to the Nb powder, while their fracture toughness at room temperature decreases. As for the Nb–Al–Mo and Nb–Al–W system, the effect of solid-solution hardening of W was larger than that of Mo, and Nb–15Al–40Mo compact has the highest strength at room temperature and 1273 K among Nb–15Al–xMo compacts.     

A study on the sintering of ultrafine grained tungsten with Ti-based additives

Tungsten (W) is a brittle material at room temperature making it very difficult to fabricate. Although the lack of ductility remains a difficult challenge, nano-sized and ultrafine grain (UFG) microstructures offer potential for overcoming tungsten's room temperature brittleness. One way to manufacture UFG W is to compact and sinter nanosized W powder, however, it is a non-trivial task to control grain growth during sintering. In an effort to inhibit grain growth, the effect of Ti-based additives on the densification and grain growth of nano-W powders was investigated in this study. The addition of 1 wt.% Ti into tungsten led to more than a 63% decrease in average grain size of sintered samples at comparable density levels. It was also found that sintering in Ar yielded a finer grain size than sintering in H₂ at similar densities. Compared to conventional high temperature sintering, a lower temperature sintering cycle for a longer hold time resulted in both near-full density and fine grain size. The roles of the Ti additive include not only the inhibition of grain growth, but also the potential absorption of oxygen from W particles.     

溶胶-喷雾干燥超细/纳米晶W-20Cu复合粉末的烧结行为

采用喷雾干燥-氢气还原法制备超细/纳米晶W-20Cu(质量分数,%)复合粉末,粉末压坯直接从室温推入高温区烧结不同时间后直接取出水淬,研究其烧结致密化和显微组织的变化。结果表明,超细/纳米晶W-20Cu粉末在1000～1200℃烧结时发生迅速致密化。粉末压坯在1200℃烧结60min,其材料致密度已达到96.4%。1420℃烧结90min时致密度达到99%以上。1100～1420℃烧结时其烧结致密化活化能不断减小,从1100℃时的276.3kJ/mol减小到1420℃时的29.1kJ/mol。当温度低于1200℃时,W晶粒长大不明显,当温度超过1300℃时,W晶粒开始有明显长大。随温度的升高W晶粒发生显著球形化,1420℃烧结时发现其晶粒长大符合G3=kt的Ostwald机制,此时晶粒长大动力学系数K仅为0.024μm3/min。     

New insights into the accelerated sintering of tungsten with trace nickel addition

In Ni-doped W alloys, 1–4 wt% of Ni was often employed to accelerate densification in conventional sintering process but at the expense of restricted service temperatures because of formation of liquid phase. To break the dilemma, in this work 0.1 wt% Ni was alloyed into W matrix and achieved 98% relative density. The densification and grain growth behaviors of both pure and nickel doped tungsten compacts were investigated, in which a potential new accelerated sintering mechanism by solid-solution alloying was explored. First-principles calculations demonstrated the transition barrier for vacancies in W system was lowered by 34% upon Ni doping. This alloying process therefore was beneficial for lattice diffusion of tungsten that, in turn, improved the sintering performance and service abilities of tungsten-nickel alloy.